Treatment of organic liquids



Navig?, i945. J. L.. KELLOGG 2,389,732

TREATMENT OF ORGANIC LIQUIDS Filed Aug. 23, 1941 2 Sheets-Sheet PatentedNov. 27, 1945 2,389,732 TREATMENT or onGANIo LIQUms John L. Kellogg,Chicago, Ill., assignor, by niesne asslgnmentato John L. Kellogg & Co.,Chicago, Ill., a corporation of Illinois Application August 23, 1941,Serial No. 408,052

'7 Claims.

This invention relates to the treatment of organic liquids such asextracts of coffee and decaleinized coffee, vegetable extracts used ascoffee substitutes, tea extracts, fruit and vegetable juices, soups andmilk; and more particularly to the treatment; of such liquids inconnection with the condensing or evaporation of the same for theproduction of evaporated, condensed or powdered products; and theprimary objects of the invention are to improve the keeping quality ofsuch products, and, particularly in the case of condensed or evaporatedliquids, to effect the retention and preservation of the originalflavors and aromas of the organic material, solid or liquid, from whichthe extract or evaporated' or condensed product is made, whichfiavorsand aromas are likely to be lost or destroyed in part during thecondensing, evaporating or drying operations.

To these ends the invention contemplates certain procedures which arecapable of being used separately but are preferably used in conjunctionone with the other as follows:

(1) The liquids, particularly, fruitr and vegetable juices and milk, arepreferably treated with a small quantity of taka-diastase, an enzymederived from the fungus species Eurotium oryzae (United States patent toTakamine et al., No. 1,391,219, September 2, 1921) for the purpose ofinhibiting or arresting bacterial action tending to bring aboutdeterioration or spoiling of the organic liquids. The use oftaka-diastase in the production of coffee extracts, for the solubilizingeffect on the carbohydrate or related constituents of the coffee, isdisclosed in applicants co-pending application Serial No. 362,819, filedOctober 25, 1940, now Patent No. 2,281,138, and application Serial No.412,898, filed September 29, 1941, now Patent No. 2,282,139, and theseparticular treatments are not specifically claimed herein.

In place of using taka-diastase other diastatic enzymes or substancescontaining diastatic enzymes might be used provided the use of suchmaterial does not detrimentally affect the taste of the product. Maltextract in most cases is not desirable because of the characteristictaste which it produces.

(2) If the organic liquid is to be condensed or evaporated at relativelyhigh temperature, for

example, in a vacuum pan, there is added to the heavy extract from thevacuum pan, a light extract or juice, for example, an extract made byfreezing fresh material or making an extract therefrom with or withoutconcentration at low temperature but above the freezing point; and iffurther evaporation is contemplated, for example, if the material is tobe evaporated to dryness, the density of the mixture is calculated so asto be suitable for instantaneous drumor spray drying, whereby thevolatilization of the taste and aroma giving constituents of thematerial during the final evaporation stage is minimized.

ture has restored to it the qualities removed or of orange juice, etcetera.

destroyed, orlpartially removed or destroyed, by the treatment in thevacuum pan.

(3) To further preserve and effect the retention of these taste andaroma giving substances, there is preferably mixed with the liquid, whenthis liquid is to be evaporated to dryness, a small quantity of avegetable oil, preferably hydrogenated in part or wholly, and preferably. though not necessarily consisting, in part or wholly, of oilderived from the material treated, e. g., coffee oil in case of coffeeextracts, orange oil in case The oil is added to the mixture of lightand heavy extracts, or to one or other of the constituent extractsbefore the extracts are subjected to the final drying operation. Thefunctions of the oil, which is used in relatively small quantities, arefirst to retain flavor and aroma; and second to stop dust formation inthe drying and subsequent treatment, grinding, for example, of theproduct.

(4) In the co-pending application of applicant, Serial No. 362,819, ledOctober 25, 1940, is disclosed an extracting process, intendedparticularly for the production of soluble coffee extracts in which thecoffee material is given successive extracting operations, with heat andagitation, in which process the extracts Imove in countercurrent to thecoiee material. In this application there is also disclosed a cookingstep in which the material, before it enters the last extractingoperation, is cooked under steam pressure so as to make possible theremoval of additional extractives in the extracting operation whichfollows-extractives which would not be removable by the usual extractionoperation except for the cooking step-and thereby increase yields. Theapplicant has since discovered that the cooking step which does notinvolve agitation, or but little agitation, is more advantageously usedat the stage of the process which gives the final extract going to thevacuum pan, which will be referred to, rather arbitrarily, as the No. lextract, meaning the extract from the first treatment of the material inthe counter-current extracting system. By cooking the co'ee material(which will preferably, as a matter of economy, be the material fromwhich the preliminary or low temperature extract has been made) withoutthis cooking step being followed by an extracting operation withagitation, a clearer extract is obtained than with the process ofapplication Serial No. 362,819. where three extractions, with agitation,are made after the material has been cooked. The cooking coagulatescolloids which may then be removed by filtration or centrifuging.

The invention is exemplified in the following specific examples which,however, should be regarded as typical and informative only and not aslimiting the invention to the particulars given therein; the intentionbeing to cover all equivalents of the process steps described and alsoall modifications of such processes within the scope of the heretoappended claims.

In the drawings are illustrated certain of the specific examples.

Figure 1 is a flow sheet illustrating the process of the presentinvention as applied to the production of coffee extracts.

Figure 2 is a flow sheet illustrating the process as applied to theproduction of extracts from fruits or vegetables, specifically to theproduction of concentrated tomato juice; and

Figure 3 is a flow sheet illustrating the process as applied to theproduction of condensed, evaporated or powdered milk.

Example I-Process as applied to the production of coffee extracts. Flowsheet, Figure 1.-35 pounds of roasted and ground coffee is introducedinto a vessel III with 10 gallons of fresh, cold water. The material isallowed to soak in vessel I for about one hour. The material is thensubjected to a separating operation, preferably by means of a centrifugeII. The extract from centrifuge I I is then frozen at I2, the icecrushed at I3, the crushed ice centrifuged at I4, the liquid frozenagain at I5, the ice crushed at I6 and the crushed ice centrifuged atI1. 'I'he freezing, crushing and centrifuging operations may be repeatedas often as desired in order to obtain as concentrated an extract as maybe found necessary. rI 'he operations described will give an extracthaving a density of about 15 to 20 Baume; although to obtain thisdensity a. third freezing operation may be required. The ice fromcentrifuges I4 and I'I is returned by line I8 to the fresh water supplyI9 for the soaking vessel I ll-the specified 10 gallons of fresh waterincluding the water from the returned ice. The low temperature extractfrom the centrifuge I'I is preferably clarified in a clarifyingcentrifuge 20, or otherwise by filtration, and is mixed with the No. 1extract produced by the counter-current extraction apparatus illustratedat the righthand side of the flow sheet. The coffee material fromcentrifuge II goes through line 2I (fresh coffee may be added ifdesired) to the steam cooker 22 which is provided with a steam coil 23or other suitable heating means. 'I'he coii'ee material mixed with No. 2extract through line 24 is brought to a boil and boiled for about 5minutes. The material is then centrifuged at 25, and the coiiee materialintroduced into the extracting vessel 26 which is provided with anagltator 21 and a steam coil 28. The mixture of coffee material fromcentrifuge 25 and No. 3 extract through line 29 is maintained at atemperature of about 125 F. (120-l30) for one hour with agitation. Thematerial is then centrifuged at 30, the liquid. No. 2 extract, goingthrough line 24 to cooker 22 as described, and the solids to theextracting vessel 3| provided with agitator 21 and steam coil 28, intowhich is introduced about 10 to 13 gallons of fresh water and about 1Aounce of taka-diastase in the powdered form. The extraction proceeds ata temperature of about 125 F. for one hour. with agitation; after whichthe material is centrifuged at 32, the spent grounds being discharged at33 and the liquid,

No. 3 extract, through line 29 to the extracting vessel 26. Iheextraction at about 125 F. (120- 130) is for the purpose of giving anoptimum temperature for action of the taka-diastase.

Obviously the process might employ Aa larger number of extractingoperations.

The No. 1 extract from centrifuge 25 is preferably clarified in theclarifying centrifuge 34 and is then introduced into the vacuum pan 35,operating, for example, at a vacuum of 28 inches of mercury, in whichthe extract is evaporated to a density of about 30-32 Baum. Preferably,and particularly if the extract is to be evaporated to dryness, there isadded to the evaporated extract at 36 (or to the extract going to thevacuum pan 35) about 1/2 ounce of hydrogenated oil, which may be coffeeoil or any hydrogenated vegetable oil, which, in the amount used, doesnot affect the taste of the extract. The addition of the hydrogenatedoil to the material in process is not covered generically herein as itis disclosed or claimed in applicant's co-pending application, SerialNo. 375,542, filed January 21, 1941. The use of the oil is claimedherein only as the stage of the process and for the purposes specied.

The low temperature extract from the freezing operations is mixed at 31with the concentrated extract from the counter-current extractingsystem. This mixture may be packaged and sold as a liquid or semi-liquidextract, or it may be subjected to a drying operation, preferably of theinstantaneous type. The drawings indicate a pair of drying rolls 38, 38,into the bight oi' which is introduced the liquid from mixer 31. Therolls will, of course, be provided with the usual doctor blades forscraping oil the material, which may then be reduced to a powder in thepulverizer 39. A single drying roll may be used, in which case thedensity of the extract mixture need not be quite as high as indicated.That is, it may be possible to omit some or all of the freezingoperations. It will also be possible to use spray drying instead ofdrying upon roll or rolls.

By employment of the process as described, the final extract willcontain extractives, of a more or less volatile character and resultingfrom the preliminary low temperature extracting operation, to compensatefor the removal, destruction or deterioration of correspondingconstituents of the coffee material which occur as a consequence of therelatively high temperatures prevailing in the counter-currentextracting system and also in the vacuum pan employed for evaporating orconcentrating the extract from the counter-current extracting system. Inthis way, without sacrifice of yields, the extract has the flavor andaroma of the original coffee material.

Example Z-Modifled coilee emtraction procesa-Instead of using freshwater in the preliminary low temperature extraction and concentratingthe extract by freezing, it will be possible to omit the freezingoperations and obtain an extract of suiliciently high density by using,instead of fresh water, for the preliminary soaking operation, anextract from the counter-current extracting system. Or this expedientmay be combined with the freezing process.

In any case, a low temperature extract or juice containing extractivespreserved. because of the low temperature, is mixed with the moreconcentrated extract obtained through the use 0f relatively hightemperatures, so as to give the final extract mixture extractives of acharacter which the extract from the usual coffee extracting system doesnot have, or in which it is more or less decient. because of 'the hightemperatures at which the entire materialA is subjected. The employmentof diastase in connection with the extraction requires a temperaturefavorable to the enzymes, and at this temperature certain extractivesare driven off or destroyed, partially or wholly. This effect takesplace to a greater extent in the vacuum pan. The resultant deficiency inthese extractives is compensated for by the addition of the lowtemperature extract.

Example 3-Fruit or vegetable juice (tomato juice), Figure 2.-100 poundsof tomatoes are pulped at 30 by any suitable pulping apparatus and thejuice frozen at di. The ice is crushed at l2 and centrifuged at $3. Theliquid from the centrifuge 133 is frozen at d, crushed at 135, andcentrifuged at 46. The freezing, crushing and centrifuging operationsmay be repeated as often as necessary or desirable in order to obtain anextract of high density as Working conditions may require. This lowtemperature extract may have a density of 15-20 Baum. The pulp from thepulping operation at 40 is introduced through line 4l into the mixer 48,together with the ice from centrifuges 43, 46 through lines 49, 50.About A of an ounce of powdered taka-diastase is preferably introducedinto the mixer 48 and the mixture 'heated to a temperature of about 125F. (12W-130 F.) for about vone hour. The material from mixer 48 iscentrifuged at 5l and the spent pulp discharged from the process; or itmay be retreated. The juice from centrifuge 5I is concentrated in thevacuum pan 52, preferably operating at a vacuum of 28 inches of mercury,to a density of -30 Baum. The concentrated extract from the vacuum pan52 is mixed at 53 with the low temperature extract from centrifuge 48.This mixture may be bottled or canned or, for a dry product, may bedried on the drying rolls 5B, 54 and powdered in the Dulverizer 55.

f the vegetable or fruit juice treated in accordance with this exampleis to be dried to a powder, asset 11e to A of 1%, based upon the weightof the extract, of a hydrogenated vegetable oil, is introduced into themixer 53 to prevent the volatilization of extractives in the dryingoperation at 54, 54. It is not necessary that all of the oil used behydrogenated. Enough, say 1A, should be hydrogenated in order to preventthe development of rancidity.

Example 4Soup procesa-The process illustrated in Figure 2 may be adaptedto the manufacture of soups by introducing into mixture 48 the ordinarysoup ingredients; vessel 48 being, in this case, the soup kettle. Theflavor of the soup is improved -by the ultimate introduction thereintoof the low temperature extract.

Example 5-Condensed, evaporated or powdered milk, Figure 3 10 gallons oimilk are frozen at 51. the ice crushed at 58, and centrifuged at 59. Theliquid is frozen at 60 and the ice crushed at 6I and centrifuged at 62.The freezing, crushing and centrifuging operations may be repeated asoften as may be required. The ice from centrifuges 59 and 62 isintroduced through lines 63, 84. into the vacuum pan 65 into which isalso introduced, preferably, l0 gallons of fresh milk. The vacuum panmay operate at a vacuum of 28 inches of mercury and the milk isthickened to a density 0f about 2030 Baum. The ice extract, in line 66,which may have a density of 12-20 Baume, is introduced with the.partially evaporated milk from the vacuum pan 65, through line 61 intothe heater 68 through which is introduced :di of an ounce oftaka-diastase, which serves not only to soften the casein but topreserve the milk. The mixture is heated to a temperature of 125 F. -forabout one hour with agitation.

In the case of condensed milk, sugar may be.

added as is customary. The mixture from the heater 68 may be bottled orcanned, or may be dried on the drying rolls 69, B9 and powdered inpulverizer 1G.

As in the other processes a small quantity of hydrogenated oil may beintroduced into the mixture before drying on the rolls 59, E9.

No claim is made specifically to the herein described processes .for theproduction of coffee extracts as these processes are covered bycopending .application of the applicant, led September 2l, 1942, as acontinuation-in-part hereof, as Serial No. 459,104.

I, claim:

1. Treatment of an edible liquid selected from liquids of animal andvegetable origin to inhibit detrimental bacterial action whichcomprises: incorporating in and reacting with the liquid a small amountof taka-diastase.

2. Treatment of an edible liquid selected from liquids of animal andvegetable origin to inhibit detrimental bacterial action whichcomprises: incorporating in the liquid a small amount of takadiastaseand agitating the liquid at a temperature of about -130 F.

3. Treatment of an edible liquid selected from l liquids of animal andvegetable origin to inhibit detrimental bacterial action whichcomprises: incorporating in and reacting with the liquid a small amountof a tasteless dlastase.

4. Treatment of selected juices of vegetable and animal origin toprevent deterioration which comprises: incorporating in and reactingwith said juices a small amount of taka-diastase and maintaining thematerial at a temperature favorable to the action of dlastase.

5. Improved process of making edible extracts from selected vegetableand animal materials which comprises: making a concentrated extract fromthe selected material by prolonged cooking at relatively hightemperatures; adding to said concentrated extract a concentrated extractof like material made at a freezing temperature; and subjecting themixture to a substantially instantaneous drying operation to evaporatemoisture therefrom.

6. Improved process of making edible extracts from selected vegetableand animal materials which comprises: making a low temperatureconcentrated extract from the selected material by freezing the same;making a concentrated extract from the residual material by prolongedapplication of heat; and mixing these extracts.

7. Improved process of making edible extracts from selected vegetableand animal materials which comprises: making a low temperature extractfrom the selected material by freezing the same and removing the icecrystals from the heavier liquid; making a concentrated extract from theresidual material by prolonged application of heat; mixing theseextracts; and subjecting the mixture to a substantially instantaneousevaporating operation to reduce the mixture to substantial dryness.

'OHZN L. KELLOGG.

